Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PCBs, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in terms of providing them with appropriate matrix CRMs enabling the process of quality control. NMIs and DIs with proven metrological capabilities for the production and certification of such materials are necessary for the provision of quality data. This project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Production process includes good manufacturing practices for processing materials, method development and validation for homogeneity, stability and characterisation tests, characterisation of selected analytes together with additional information about matrix constituents, the calculation of individual uncertainties (between units inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. Inter laboratory comparison registered as EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills.

Within a class of agrochemical residues, pesticides are significant concern due to their various adverse effects on people, animals and the environmental systems. Once they entered to food or to the environment, the parent compound is transformed to metabolites which have different toxicity profiles. Activities like food cooking and waste water treatment (WWT) may lead to produce more toxic metabolites than the parent substances.
Online coupling of electrochemistry with liquid chromatography mass spectrometry (EC-HPLC-MS) is one of the most promising and powerful techniques for metabolite studies which exploited widely for pharmaceuticals so far [1]. However, data on the application of EC-HPLC-MS to simulate environmental transformation products, the fate of contaminants and their metabolic pathways are rare. The oxidation of analyte of interest on the EC, separate the metabolites on HPLC and identifying them by MS gives enormous advantages to identify the contaminants transformation products [2]. Thus, applying this technique (EC-MS, EC-HPLC-MS, and HPLC-EC-MS) for transformation products of pesticide residues is urgently needed.
The main interest of this study will be investigating the electrochemical oxidative degradation products, simulating to in-vitro metabolites and transformation processes of selected pesticides in food and environmental samples. The parent pesticides’, like carbamates and abamectin, oxidation by EC, product metabolites identification and their fates will be discussed using electrochemistry coupled to HPLC-MS techniques.

This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills.

Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PFOS, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in order to establish a quality system. It is necessary to provide appropriate calibrators i.e. matrix CRMs relates to the unique sample matrices representing typical samples in the geomorphological and anthropological sense. In addition to that, bearing in mind the complexity and instability of environmental samples, it is very difficult to obtain appropriate referents materials with no local providers.
Our project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Our project will have an impact on environmental monitoring in the partnering countries and on the scientific community, who will use the newly developed reference materials. Furthermore, partners will develop strategies for producing new CRMs either on their own or in cooperation. This will lead to regional CRM producers serving scientific and official laboratories.

While organic pollutants have been extensively studied in urban and agricultural areas, data from forested regions are relatively rare.
Within the framework of a forest soil inventory in Germany polycyclic aromatic hydrocarbons (PAH), polychlorinated biphenyls (PCB) and organochlorine pesticides (OCP) were analyzed in 1500 soil samples taken from 3 soil horizons at 447 sites. An analytical protocol was developed and validated for the simultaneous extraction and measurement of all analytes in humic rich soil at trace level range. It included pressurized liquid extraction (PLE) and a two step cleanup procedure consisting of gel permeation chromatography (GPC) followed by solid phase extraction (SPE). Quantification was carried out using gas chromatography combined with mass spectrometry (GC-MS). In line with the monitoring campaign a comprehensive quality assurance concept was implemented to guarantee constant analytical measurement conditions for two years. The protocol is applicable for field laboratories with a high level of automation and for analyzing high sample amounts.
At most sampling sites pollutant concentrations gradually decrease with depth. Only few spots showed highest concentrations in the upper mineral soil. In the O-horizon the sum concentrations of 16 PAHs range from 104 to 14.000 µg/kg, of 6 PCBs from <1 to 106 µg/kg and the sum of DDT and metabolites range from <1 to ca. 4.000 µg/kg.
The observed concentration of PAH, PCB and OCP reflect an ubiquitous background contamination at most sites. Relatively high concentrations of PAH and PCB are related to industrial areas and peak concentrations only of PAH are associated with open cast mining of brown coal areas. The spatial distribution of the contents of DDT and metabolites in German forest soils can clearly be attributed to historic application. A contribution of ubiquitous background pollution derived from long-range atmospheric transport is likely for some compounds in the studied area, e.g., DDT in the western part of Germany. The results generally reflect the distribution of POPs in densely populated and industrialized countries located in temperate regions].

The occurrence of persistent organic pollutants like polychlorinated biphenyls (PCB) and organochlorine pesticides (OCP) in the environment is still a matter of concern, even years after their use was abolished. Hence, threshold values are regulated by law which reference a number of national and international standards for determination of said contaminants. In this context, soil is an especially difficult matrix, because several defining parameters can vary in a wide range. Organic matter content in particular has a crucial influence on extractability of contaminants because it largely governs formation of non-extractable or bound residues.
For this study, four soils of different total organic carbon (TOC) content were generated from uncontaminated reference soil (RefeSol 01-A) and compost which were spiked to contaminant levels representative of the Bundes-Bodenschutz-Verordnung (BBodSchV). These test materials were extracted using accelerated solvent extraction (ASE), Soxhlet extraction, and liquid-liquid extraction. For the latter method, samples were initially extracted for 15 minutes employing acetone. The follow-up extraction step was carried out using cyclohexane and the extraction time varied between 15 minutes and 16 hours. After clean-up, extracts were analysed via gas chromatography-mass spectrometry (GC MS) and with a gas chromatograph equipped with an electron capture detector (GC ECD).
Statistical analysis of the experimental values showed that recovery was not dependent on matrix TOC content. Also, no clear preference for a single method could be detected. Concerning liquid-liquid-extraction, it is merely observed that prolonged extraction time results in slightly higher recoveries, while moderate extraction times appear to yield the most robust results. Although Soxhlet and ASE show high recoveries, they also lead to larger standard deviations and are not suitable for determination of thermolabile pesticides.
In addition to recovery by different extraction methods, the agreement of values obtained by ECD and MS was evaluated. For ECD, standard deviations are generally higher but overall the values obtained by MS and ECD are comparable.

A 400 m² soil test field with gas injection system was built up, which enables an experimental validation of linear gas sensors for specific applications and gases in an application-relevant scale. Several injection and soil watering experiments with carbon dioxide (CO2) at different days with varying boundary conditions were performed indicating the potential of the method for, e.g., rapid leakage detection with respect to Carbon Capture and Storage (CCS) issues.

This project aims to develop capacity to produce certified reference materials (CRMs) for environmental analysis by transferring know-how between the partners and combining their skills to focus on environmental CRM production. The production process includes good manufacturing practices for processing materials, method development, the validation and application of homogeneity, stability and characterisation tests, the calculation of individual uncertainties (between-unit inhomogeneity, long term stability, characterisation) and combination of uncertainties to determine overall uncertainty of the matrix reference materials. An inter laboratory comparison registered as a EURAMET project is set as the ultimate project outcome, confirming the partners’ capabilities in applying newly acquired skills.

Reliable analysis of chemical indicators in water, sediment and soil samples for the purpose of environmental pollution assessment poses one of the greatest analytical challenges, having in mind the complexity of sample matrix and low concentrations of pollutants. Organics (pesticides, PAHs, PFOS, etc.) and heavy metals (Hg, Cd, Ni, Pb and As) represent target parameters. Laboratories performing sampling and tests in this field regulated by respective EU directives, need strong support in order to establish a quality system. It is necessary to provide appropriate calibrators i.e. matrix CRMs relates to the unique sample matrices representing typical samples in the geomorphological and anthropological sense. In addition to that, bearing in mind the complexity and instability of environmental samples, it is very difficult to obtain appropriate referents materials with no local providers.
Our project is aiming to develop capacity to produce CRMs for environmental analysis by transferring the theoretical and practical know-how between the partners and combining their skills to focus on environmental CRM production in accordance with ISO Guide 34. Our project will have an impact on environmental monitoring in the partnering countries and on the scientific community, who will use the newly developed reference materials. Furthermore, partners will develop strategies for producing new CRMs either on their own or in cooperation. This will lead to regional CRM producers serving scientific and official laboratories.